CN111689848B - Method for recycling and purifying wastewater containing maleic acid - Google Patents
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Abstract
The invention discloses a method for recycling and purifying wastewater containing maleic acid, which comprises the steps of taking a bromine-containing compound and peroxide as phase transfer catalysts, converting maleic acid in the wastewater containing the maleic acid into fumaric acid through an isomerization reaction, and carrying out solid-liquid separation to obtain a crude product of the fumaric acid; heating and dissolving the crude fumaric acid in a solvent, thermally decoloring by using activated carbon, recrystallizing, and drying to obtain a refined fumaric acid product; performing regeneration treatment on the activated carbon; and (3) the wastewater after the fumaric acid crude product is separated, pollutants generated by activated carbon regeneration treatment and gas generated by drying enter an oxygen-critical cracking device for purification treatment. The invention uses bromine compound and peroxide to form phase transfer catalyst, while the yield of fumaric acid can reach 90%. Meanwhile, the wastewater from which the fumaric acid crude product is separated after isomerization, the methanol-containing polluted gas generated in the drying process and the pollutants generated by the regeneration treatment of the activated carbon are sent to an adjacent oxygen cracking device for purification treatment, so that pollution-free clean production is realized in the process of producing the fumaric acid from the maleic acid wastewater.
Description
Technical Field
The invention belongs to the field of treatment of wastewater containing maleic acid, and relates to a recycling and purifying treatment method of wastewater containing maleic acid.
Background
In the production process of phthalic anhydride, a large amount of wastewater with the maleic acid mass fraction of about 10-25% is produced as a byproduct, and the maleic acid is converted into fumaric acid by an isomerization method. Fumaric acid has many uses, and can be used for producing L-aspartic acid, ferrous fumarate, unsaturated polyester resin and fumaric acid esters.
The patent CN104045550A discloses a fumaric acid production process, which comprises the steps of firstly carrying out decoloration treatment on maleic acid wastewater, then converting the maleic acid wastewater into fumaric acid by using urea and diammonium hydrogen phosphate as catalysts, wherein the product yield can reach 95-99%, and the product is pure white. Patent CN103204773A discloses a method for preparing fumaric acid by cis-trans isomerization of maleic acid, which comprises the step of carrying out catalytic isomerization on maleic acid serving as a raw material in a DMF (dimethyl formamide), DMSO (dimethyl sulfoxide), ethyl acetate, benzene, toluene or nitrobenzene solvent in the presence of air or oxygen under the conditions of 50-150 MPa, 0.1-1.2 MPa and a raw material-solvent mass ratio of 1: 1-1: 80 to obtain fumaric acid, wherein the yield can reach more than 85%. Patent application CN104016852A discloses isomerizing maleic acid wastewater into fumaric acid under the catalysis of thiourea at 50-100 ℃, crystallizing to obtain a crude fumaric acid product, dissolving the crude product in water, decoloring, crystallizing and drying to obtain a product, wherein the adopted decoloring agent is polymeric aluminum ferric chloride, activated carbon, activated resin, activated clay, activated sand and a combination thereof, the fumaric acid product is dried in vacuum, and the purity of the product is 99.8-99.9%. The technical scheme can only realize isomerization to obtain fumaric acid, does not provide how to purify and treat isomerized wastewater, and cannot really realize the recycling and purification treatment of wastewater containing maleic acid, and the isomerized wastewater contains metal ions or sulfur elements, for example, the metal ions can deposit to influence the treatment effect, and the sulfur elements can poison the catalyst to influence the wastewater treatment.
Disclosure of Invention
The invention aims to provide a recycling and purifying treatment method for wastewater containing maleic acid formed after absorbing tail gas of phthalic anhydride oxidation reaction by water.
The purpose of the invention can be realized by the following technical scheme:
a method for recycling and purifying wastewater containing maleic acid takes a bromine-containing compound and peroxide with peroxy-O-O-as phase transfer catalysts, maleic acid in the wastewater containing maleic acid is converted into fumaric acid through isomerization reaction, and a crude fumaric acid product is separated from the wastewater by solid-liquid separation by utilizing the solubility difference of the maleic acid and the fumaric acid in water, so that the recycling of the maleic acid is realized; heating and dissolving the crude fumaric acid in a solvent, thermally decoloring by using activated carbon, recrystallizing, and drying to obtain a refined fumaric acid product; and (3) carrying out regeneration treatment on the wastewater and the activated carbon after the fumaric acid crude product is separated out, and enabling pollutants generated by the regeneration treatment of the activated carbon and gas generated by drying to enter an oxygen cracking device and be purified under the action of an oxygen cracking catalyst, so that the wastewater and the waste gas are discharged up to the standard.
The wastewater containing maleic acid is formed by absorbing phthalic anhydride oxidation reaction tail gas with water, and the mass fraction of maleic acid in the wastewater is 8-28%.
The phase transfer catalyst of the present invention is composed of a bromine-containing compound and a peroxide. The bromine-containing compound is selected from one of tetraethylammonium bromide, tetrapropylammonium bromide, tetrabutylammonium bromide, dodecyltrimethylammonium bromide, hexadecyltrimethylammonium bromide and octadecyltrimethylammonium bromide; the peroxide is selected from one of benzoyl peroxide, tert-butyl peroxide, cumyl peroxide, benzoic peroxide and hydrogen peroxide. The phase transfer catalyst does not contain inorganic metal ions, so that the possibility of generating inorganic salt during the purification treatment of the waste water after isomerization is avoided. Because the solubility of the peroxide in water is far less than that of maleic acid (the solubility of maleic acid in water is 788g/L), and the catalytic isomerization reaction is carried out in the water phase, the peroxide cannot directly collide with the maleic acid molecules to play a catalytic role, so that the bromine-containing compound with the phase transfer capability is selected, and the peroxide is transferred to the water phase to catalyze the isomerization of the maleic acid.
The dosage of the bromine-containing compound is 0.1-2 wt% of the mass of the wastewater, and the dosage of the peroxide is 0.5-10 wt% of the mass of the wastewater.
The temperature of the isomerization reaction is 55-95 ℃.
After isomerization reaction, crude fumaric acid can be separated out by filtering, and COD of wastewater after the crude fumaric acid is separated out is 150000-250000 mgO2In addition to part of the fumaric acid still dissolved in the aqueous phase, there are also organic heteropolyacids such as benzoic acid and phthalic acid which are formed during the oxidation reaction of phthalic anhydride.
The solvent is a mixed solution of methanol and water in a mass ratio of 50: 50-90: 10.
And dissolving the crude fumaric acid in a solvent at the temperature of 55-75 ℃.
The temperature of thermal decoloring is 55-75 ℃.
The recrystallization temperature is 15-30 ℃.
The temperature of the activated carbon regeneration treatment is 250-650 ℃, the vacuum degree is 0.095-0.099 MPa, and the regeneration time is 0.5-5 h. The regenerated active carbon is reused in a thermal decoloring working section.
As a preferable technical scheme of the method for recycling and purifying the wastewater containing the maleic acid, the recrystallization mother liquor is recycled for dissolving the crude fumaric acid.
The drying temperature is 80-100 ℃, the drying time is 3-8 hours, air is introduced in the drying process to take organic steam and water vapor generated by drying out of the system, and the pollutant in the gas generated by drying is methanol.
The catalyst for cracking oxygen is metal oxide catalyst, and ZrO is used as catalyst2、TiO2Or Ce2O3One of the two is used as a carrier, a transition metal oxide is used as an active component, and the loading capacity of the active component is 1-15%; the transition metal oxide is two or three oxides of copper oxide, nickel oxide, vanadium oxide, chromium oxide, manganese oxide and cobalt oxide. The particle size of the catalyst is 3-6 mm.
The wastewater after the fumaric acid crude product is separated is in a liquid form for 0.05-0.5 h at a mass airspeed-1The wastewater enters an oxygen cracking device, air is introduced at the same time, the feeding amount of the air is the same as the feeding volume flow rate of the gasified wastewater, and the mass airspeed of pollutants generated by activated carbon regeneration treatment is 0.005-0.05 h-1Entering an oxygen cracking device, and drying the generated gas at a volume space velocity of 2000-20000 h-1Entering an oxygen-critical cracking device; the temperature of the purification treatment is 250-400 ℃; the total content of Volatile Organic Compounds (VOCs) in the tail gas discharged from the temporary oxygen cracking device is lower than 40mg/m3The total content of Chemical Oxygen Demand (COD) in the wastewater discharged from the temporary oxygen cracking device is lower than 40 mg/L.
The invention has the beneficial effects that:
the phase transfer catalyst consisting of the bromine-containing compound and the peroxide catalyzes maleic acid to isomerize fumaric acid, the yield of the fumaric acid reaches over 90 percent, the phase transfer catalyst does not contain inorganic metal ions, the possibility of generating inorganic salt during purification treatment of waste water after isomerization is avoided, and the phase transfer catalyst also does not contain sulfur elements and does not poison the critical oxygen cracking catalyst. The method simultaneously sends the wastewater of the crude fumaric acid product separated after isomerization, the methanol-containing polluted gas generated in the drying process and the pollutants generated by the regeneration treatment of the activated carbon into the temporary oxygen cracking device for purification treatment, so that the pollution-free clean production is realized in the process of producing the fumaric acid by the maleic acid wastewater, the problem that the wastewater of enterprises for producing the fumaric acid by the maleic acid wastewater cannot be treated at present can be solved, the pollution is eliminated in the production device, and the integrated innovation of the recycling and purification treatment of the maleic acid wastewater is realized.
Drawings
FIG. 1 is a flow chart of the method for recycling and purifying wastewater containing maleic acid.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
3000kg of wastewater with maleic acid mass fraction of 10.4 percent is added with 3kg of tetraethylammonium bromide and 15kg of benzoyl peroxide, and the maleic acid is isomerized into fumaric acid by catalytic isomerization reaction at 95 ℃, wherein the yield of the isomerized fumaric acid is 91.1 percent.
Example 2
3000kg of wastewater containing 17% by mass of maleic acid was added with 4.5kg of tetrapropylammonium bromide and 120kg of hydrogen peroxide, and the maleic acid was isomerized into fumaric acid by catalytic isomerization at 80 ℃, with the yield of isomerized fumaric acid being 96.3%.
Example 3
3000kg of wastewater with maleic acid mass fraction of 28 percent is added with 30kg of tetrabutylammonium bromide and 300kg of tert-butyl peroxide, and the maleic acid is isomerized into fumaric acid by catalytic isomerization reaction at 55 ℃, wherein the yield of the isomerized fumaric acid is 93.8 percent.
Example 4
3000kg of wastewater with maleic acid mass fraction of 8 percent is added with 60kg of dodecyl trimethyl ammonium bromide and 30kg of peroxybenzoic acid, and the maleic acid is isomerized into fumaric acid by catalytic isomerization reaction at 60 ℃, wherein the yield of the isomerized fumaric acid is 90.6 percent.
Example 5
3000kg of wastewater with maleic acid mass fraction of 22 percent is added with 15kg of hexadecyl trimethyl ammonium bromide and 150kg of cumyl peroxide, and the maleic acid is isomerized into fumaric acid by catalytic isomerization reaction at 90 ℃, wherein the yield of the isomerized fumaric acid is 98.2 percent.
Example 6
3000kg of wastewater with maleic acid mass fraction of 22 percent is added with 45kg of octadecyl trimethyl ammonium bromide and 90kg of hydrogen peroxide, the catalytic isomerization reaction is carried out at 88 ℃ to isomerize the maleic acid into fumaric acid, and the fumaric acid crude product is obtained by cooling and filtering after the reaction is finished, wherein the yield of the fumaric acid is 96.9 percent. And (5) purifying the filtrate in an oxygen-critical decomposition device.
Taking 500kg of crude fumaric acid, dissolving the crude fumaric acid in a solvent consisting of 375kg of methanol and 375kg of water under stirring at 70 ℃, adding 2.5kg of activated carbon, continuing stirring for 1h at 70 ℃, filtering while hot to obtain 5.25kg of wet activated carbon, cooling the filtrate to 30 ℃, recrystallizing to separate out fumaric acid crystals, filtering to obtain 448.1kg of white crystals (carrying 10.9kg of methanol and 13.1kg of water), introducing air, drying at 110 ℃ to obtain refined fumaric acid (the purity is 97.2%), adding 364.1kg of methanol, 361.9kg of water, 0.2kg of impurities and 36.7kg of fumaric acid in recrystallized mother liquor, and reusing the refined fumaric acid in dissolving the crude fumaric acid.
The wet activated carbon is thermally regenerated under the conditions that the vacuum degree is 0.098MPa and the temperature is 550 ℃, and the air speed of pollutant-containing gas generated in the thermal regeneration process is 0.05h-1Purifying in an oxygen cracking device filled with 1 wt% V catalyst2O5-12wt％MnO2-2wt％Co3O4/ZrO2Simultaneously, the gas generated in the fumaric acid drying process is 20000h-1Introducing into an oxygen cracking device at a volume space velocity, and filtering the isomerized filtrate for 0.5h-1Introducing mass airspeed into an oxygen cracking device, introducing air simultaneously, wherein the feeding amount of the air is the same as the feeding volume flow rate of the gasified filtrate after isomerization, purifying at the temperature of 380 ℃, and the content of gas-phase VOCs at the outlet of the oxygen cracking device is 3.9mg/m3And the COD of the discharged aqueous phase is 23mgO2and/L, the simultaneous treatment of waste gas and waste water is realized.
Example 7
The crude fumaric acid was obtained from the waste water containing 22% by mass of maleic acid by the method of example 6.
500kg of crude fumaric acid was taken, dissolved in a solvent composed of 1250kg of methanol and 125kg of water with stirring at 55 ℃, 0.5kg of the thermally regenerated activated carbon of example 6 was added, stirring was continued at 55 ℃ for 1 hour, hot filtration was carried out to obtain 1kg of wet activated carbon, the filtrate was cooled to 15 ℃, recrystallization was carried out to precipitate crystals of fumaric acid, filtration was carried out to obtain 424.5kg of white crystals, which were accompanied by 14.7kg of methanol and 4.1kg of water, air was introduced, and drying was carried out at 110 ℃ to obtain a refined fumaric acid product (purity: 98.5%). 1110.3kg of methanol, 120.9kg of water, 6.3kg of impurities and 55.3kg of fumaric acid in the recrystallization mother liquor after crystallization can be reused for dissolving crude fumaric acid.
The wet activated carbon is thermally regenerated under the conditions of vacuum degree of 0.098MPa and temperature of 650 ℃, and the air speed of the pollutant-containing gas generated in the thermal regeneration process is 0.005h-1Purifying in a temporary oxygen cracking device filled with 5 wt% CuO-5 wt% Cr2O3-2.5wt％NiO/CeO2Simultaneously, gas generated in the fumaric acid drying process is dried for 2000h-1Introducing into an oxygen cracking device at a volume space velocity, and filtering the isomerized filtrate for 0.05h-1Introducing mass airspeed into the near-oxygen cracking device, simultaneously introducing air, wherein the feeding amount of the air is the same as the feeding volume flow rate of the gasified filtrate after isomerization, purifying at the temperature of 400 ℃, and the content of gas-phase VOCs at the outlet of the near-oxygen cracking device is 5mg/m3And the COD of the discharged aqueous phase is 33mgO2and/L, the simultaneous treatment of waste gas and waste water is realized.
Example 8
The crude fumaric acid was obtained from the waste water containing 22% by mass of maleic acid by the method of example 6.
500kg of crude fumaric acid was taken, dissolved in the recrystallization mother liquor after crystallization in example 7 with stirring at 60 ℃, added with 1kg of activated carbon subjected to thermal regeneration treatment in example 6, stirred at 60 ℃ for 1 hour, filtered while hot to obtain 2.1kg of wet activated carbon, the filtrate was cooled to 15 ℃, recrystallized to separate out fumaric acid crystals, filtered to obtain 433.2kg of white crystals, which were accompanied by 8.3kg of methanol and 4.1kg of water, and air was introduced to dry at 110 ℃ to obtain refined fumaric acid (purity 96.5%).
Claims (6)
1. A method for recycling and purifying wastewater containing maleic acid is characterized in that a bromine-containing compound and peroxide are used as phase transfer catalysts, maleic acid in the wastewater containing the maleic acid is converted into fumaric acid through isomerization reaction, and a crude fumaric acid product is obtained through solid-liquid separation; heating and dissolving the crude fumaric acid in a solvent at the temperature of 55-75 ℃, and thermally decoloring, recrystallizing and drying by using activated carbon to obtain a refined fumaric acid product; performing regeneration treatment on the activated carbon; the waste water after the fumaric acid crude product is separated out is 0.05-0.5 h according to the mass airspeed-1The wastewater enters an oxygen cracking device, air is introduced at the same time, the feeding amount of the air is the same as the feeding volume flow rate of the gasified wastewater, and the mass airspeed of pollutants generated by activated carbon regeneration treatment is 0.005-0.05 h-1Entering an oxygen cracking device, and drying the generated gas at a volume space velocity of 2000-20000 h-1Entering into a temporary oxygen cracking device, purifying under the action of a temporary oxygen cracking catalyst, wherein the total content of volatile organic compounds in the tail gas discharged from the temporary oxygen cracking device is lower than 40mg/m3The total content of chemical oxygen demand in the wastewater discharged from the temporary oxygen cracking device is lower than 40 mg/L; wherein, the bromine-containing compound is selected from one of tetraethyl ammonium bromide, tetrapropyl ammonium bromide, tetrabutyl ammonium bromide, dodecyl trimethyl ammonium bromide, hexadecyl trimethyl ammonium bromide and octadecyl trimethyl ammonium bromide; the peroxide is selected from one of benzoyl peroxide, tert-butyl peroxide, cumyl peroxide, benzoic peroxide and hydrogen peroxide; the solvent is a mixed solution of methanol and water in a mass ratio of 50: 50-90: 10; the temperature of the purification treatment is 250-400 ℃; the catalyst is ZrO2、TiO2Or Ce2O3One of the two is used as a carrier, a transition metal oxide is used as an active component, and the loading capacity of the active component is 1-15%; the transition metal oxide isTwo or three oxides of copper oxide, nickel oxide, vanadium oxide, chromium oxide, manganese oxide and cobalt oxide.
2. The method according to claim 1, wherein the maleic acid-containing wastewater contains 8-28% by mass of maleic acid.
3. The method according to claim 1, wherein the amount of the bromine-containing compound is 0.1-2 wt% of the maleic acid-containing wastewater, and the amount of the peroxide is 0.5-10 wt% of the maleic acid-containing wastewater.
4. The method for recycling and purifying wastewater containing maleic acid according to claim 1, wherein the temperature of the isomerization reaction is 55-95 ℃.
5. The method for recycling and purifying wastewater containing maleic acid according to claim 1, wherein the temperature of the thermal decoloring is 55-75 ℃; the drying temperature is 80-100 ℃.
6. The method for recycling and purifying wastewater containing maleic acid as claimed in claim 1, wherein the temperature of the activated carbon regeneration treatment is 250-650 ℃, and the vacuum degree is 0.095-0.099 MPa.
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